Cure systems to eliminate restricted substances in chlorinated polymers.Historically, several products have been used to crosslink chlorinated chlorinated /chlo·ri·nat·ed/ (klor´i-nat?ed) treated or charged with chlorine. chlorinated charged with chlorine. chlorinated acids some, e.g. polymers that are now either restricted or soon to be prohibited pro·hib·it tr.v. pro·hib·it·ed, pro·hib·it·ing, pro·hib·its 1. To forbid by authority: Smoking is prohibited in most theaters. See Synonyms at forbid. 2. for use by the automotive original equipment manufacturers. Compounds containing lead and cure systems based on thiourea thiourea a goitrogenic agent used in industry as a photographic fixative. Mode of action is as for thiouracil. dominate the existing literature as recommended chlorinated polymers cure strategies. Recent automotive OEM (Original Equipment Manufacturer) The rebranding of equipment and selling it. The term initially referred to the company that made the products (the "original" manufacturer), but eventually became widely used to refer to the organization that buys the products and directives have restricted the use of lead-based curatives and several are planning on prohibiting their use in the near future. Long-term Long-term Three or more years. In the context of accounting, more than 1 year. long-term 1. Of or relating to a gain or loss in the value of a security that has been held over a specific length of time. Compare short-term. studies around the use of thiourea curatives may also restrict them in the near future. With the advent of the restricted substances material specifications now being enforced by the various automotive manufacturers, alternative cure systems must be found quickly to meet their requirements. A group of chemicals has been found that can be used to replace both the lead-based and the thiourea-based cure systems of the past. These new curatives can be used to develop compounds that are now both processable and meet the demanding performance of future specifications without using products that are restricted, soon to be prohibited or might be restricted in the future. This article will show examples of how to develop alternate cure systems for chlorinated polymers using non-restricted curatives. In 2000, the European Union European Union (EU), name given since the ratification (Nov., 1993) of the Treaty of European Union, or Maastricht Treaty, to the European Community issued a directive restricting the use of certain materials in automotive applications. These restrictions were based on the end of life vehicle (ELV ELV End-of-Life Vehicles ELV Expendable Launch Vehicle ELV Extra Low Voltage ELV Emission Limit Value (environmental protection) ELV Elektronisches Lastschrift Verfahren (German method of payment) ) requirements that regulated the recycling recycling, the process of recovering and reusing waste products—from household use, manufacturing, agriculture, and business—and thereby reducing their burden on the environment. of all parts of the automobile. Certain heavy metals heavy metals, n.pl metallic compounds, such as aluminum, arsenic, cadmium, lead, mercury, and nickel. Exposure to these metals has been linked to immune, kidney, and neurotic disorders. , including lead, were listed as restricted chemicals and after July July: see month. 1, 2005 (ref. 1), these were no longer being allowed in cars being made for and sold in the European Union. The effect on rubber compounding is that the historical curing systems for many chlorinated polymers required lead based components for acid acceptance and heat aging stability. The obvious response to this problem is to change the cure systems over to conventional thiourea systems, but there are also reports that thiourea products will also become restricted in the near future. This leaves the compounder in a significant dilemma. How can one obtain the performance properties, processing requirements and maintain compound cost control without the availability of either lead or thiourea curing components? Requirements of the new cuirng system The first criteria for a non-lead cure system are components (or variations of these components) of the new curing system must be able to cure all chlorinated polymers. This presents a significant problem because of the wide variety of chlorinated polymers now in use in automotive applications. CR, CIIR CIIR Catholic Institute for International Relations CIIR Center for Intelligent Information Retrieval CIIR counterintelligence information report (US DoD) CIIR Canadian International Information Resource , CO, ECO E·co , Umberto Born 1932. Italian writer best known for his novels, including The Name of the Rose (1981). He has also written extensively on semiotics and British and American popular culture. , ACM (Association for Computing Machinery, New York, www.acm.org) A membership organization founded in 1947 dedicated to advancing the arts and sciences of information processing. In addition to awards and publications, ACM also maintains special interest groups (SIGs) in the computer field. and others all must be curable cur·a·ble adj. Capable of being cured or healed. using the new system for it to be capable of replacing the conventional lead and thiourea systems. The new cure system needs good processing safety, needs to retain excellent heat resistance, and needs to maintain its oil and fuel resistances, all at moderate cost and without any potential for restriction of use in the foreseeable fore·see tr.v. fore·saw , fore·seen , fore·see·ing, fore·sees To see or know beforehand: foresaw the rapid increase in unemployment. future. Various cure systems exist that could meet these requirements for curing chlorinated polymers, but finding a candidate system that can meet all of the requirements could be difficult. Rhein Rhein: see Rhine, river. Chemie has tested several of these various cure systems and found that a cure system based on Rhenogran Triazine tri·a·zine n. 1. Any of three isomeric compounds, C3H3N3, each having three carbon and three nitrogen atoms in a six-membered ring. 2. A compound derived from one of these isomers. TM, combined with Rhenogran HPCA HPCA High-Performance Computer Architecture HPCA Health Practitioners Competence Assurance (bill, New Zealand) HPCA Himachal Pradesh Cricket Association HPCA Hippocalcin HPCA Hospice & Palliative Care Associates and other ingredients, could meet all of the requirements in the majority of the polymers listed. In this article, we will discuss the steps taken to optimize optimize - optimisation a non-lead, non-thiourea curing system for both epichlorohydrin ep·i·chlo·ro·hy·drin n. A colorless liquid, C3H5OCl, used as a solvent in making resins. and chloroprene chloroprene (klōr`əprēn') or 2-chloro-1,3-butadiene, colorless liquid organic compound used in the synthesis of neoprene and certain other rubbers. using Triazine TM-70 and HPCA-70, and showing the processing, performance properties and aging stability for each polymer system (ref. 2). Experimental data for ECO Using the triazine system in ECO fuel hose compounds One of the most difficult chlorinated polymers to compound is epichlorohydrin (ECO). Compounding ECO becomes even more difficult if we are to eliminate lead-based products that provide several of the important attributes to the conventional cure systems now being used. Several reference works at the end of this paper demonstrate that various forms of triazine can be used to cure ECO and other chlorinated polymers. Most of these cure systems have some type of drawback DRAWBACK, com. law. An allowance made by the government to merchants on the reexportation of certain imported goods liable to duties, which, in some cases, consists of the whole; in others, of a part of the duties which had been paid upon the importation. that prevents compounders from readily using them to meet the requirements of the new European European emanating from or pertaining to Europe. European bat lyssavirus see lyssavirus. European beech tree fagussylvaticus. European blastomycosis see cryptococcosis. directive. In the compounds developed, we will show how all of the critical properties can be achieved using a triazine cure system in ECO. Then we will show a typical chloroprene compound made with a similar curing system. The main criteria for a new ECO cure system are that they exhibit good scorch safety, are non-toxic, maintain heat resistance, produce high physical properties, have comparable mold mold, name for certain multicellular organisms of the various classes of the kingdom Fungi, characteristically having bodies composed of a cottony mycelium. The colors of molds are caused by the spores, which are borne on the mycelium. flow and are cost-effective cost-effective, n the minimal expenditure of dollars, time, and other elements necessary to achieve the health care result deemed necessary and appropriate. . One of the first challenges of using a triazine cure system to replace the traditional lead systems is that triazine cures tend to be scorchy. All tests were conducted using standard DIN and ASTM ASTM abbr. American Society for Testing and Materials procedures. In table 1, we see the effect of various retarders on a triazine cure system. The data in table 1 shows that the triazine cure system without a retarder retarder, n a chemical added to a substance to slow a chemical reaction, prolong the set of the material, and provide more working time. does not have enough shelf life to be usable USable is a special idea contest to transfer US American ideas into practice in Germany. USable is initiated by the German Körber-Stiftung (foundation Körber). It is doted with 150,000 Euro and awarded every two years. in a normal production environment. The Vulkalent E/C E/C Equipment/Component E/C Erik and Christine (Phantom of the Opera fan-fiction) E/C Engineering/Construction Contractor E/C Environment & Communications (a treated aromatic aromatic /ar·o·mat·ic/ (ar?o-mat´ik) 1. having a spicy odor. 2. in chemistry, denoting a compound containing a ring system stabilized by a closed circle of conjugated double bonds or nonbonding electron pairs, e.g. sulfonamide sulfonamide /sul·fon·amide/ (sul-fon´ah-mid) a compound containing the sbondSO2NH2 group. The sulfonamides, or sulfa drugs, are derivatives of sulfanilamide, competitively inhibit folic acid synthesis in microorganisms, and formerly were ) and B/C B/C Because B/C Broadcast B/C Boundary Conditions B/C Biological & Chemical (phthalic anhydride phthalic anhydride n. A white crystalline compound prepared by oxidizing naphthalene and used in the manufacture of phthaleins and other dyes. ) either do not retard the cure sufficiently or reduce the physical properties too much to meet the performance requirements. Only CTP CTP (cytidine triphosphate): see cytosine. (1) (Computer-To-Plate) The production of printing plates directly from the computer without requiring film as an intermediate step. (N-cyclohexylthio phthalimide Phthal´i`mide n. 1. (Chem.) An imido derivative of phthalic acid, obtained as a white crystalline substance,
Meaney spelling After adding the CTP-80 and TP-50, the compound has achieved an excellent Mooney consistency and shelf life. Now the tensile tensile, adj having a degree of elasticity; having the ability to be extended or stretched. and modulus See modulo. need to be improved to make sure that the resulting finished parts can meet the performance criteria. Adding HPCA-70 at levels of 0.5 to 0.7 phr can raise the physical properties to a level capable of meeting the automotive applications' performance requirements. In table 3, we see the effect of adding the HPCA-70 to the compound that we have been developing. Some care must be taken when adding HPCA-70, as the scorch safety can be lost if the level exceeds 0.7 pbx, as shown in the last compound in table 3. Now that we have obtained the physical properties and achieved the required processing safety, the compound must undergo aging to determine if it can sustain its performance in the harsh under-hood environments (1,000 hours at 125[degrees]C hot air aging). Table 4 shows the results of the long-term heat aging for this compound. Typical requirements for performance properties after 1,000 hours aging in hot air at 125[degrees]C include a change in hardness of less than 13 points, a minimum elongation elongation, in astronomy, the angular distance between two points in the sky as measured from a third point. The elongation of a planet is usually measured as the angular distance from the sun to the planet as measured from the earth. of 130% and a minimum tensile strength tensile strength Ratio of the maximum load a material can support without fracture when being stretched to the original area of a cross section of the material. When stresses less than the tensile strength are removed, a material completely or partially returns to its of 8 MPa. All of the triazine compounds as prepared herein show properties above the minimum requirements, with the 0.5 pbx loading of HPCA-70 showing the best combination of results and cost effectiveness. This compound is also quite cost-effective when comparing it to typical lead-based systems, since the specific gravity specific gravity, ratio of the weight of a given volume of a substance to the weight of an equal volume of some reference substance, or, equivalently, the ratio of the masses of equal volumes of the two substances. of the lead oxides is extremely high. The change to the much lower specific gravity chemicals of the triazine system significantly lowers the pound-volume cost of the entire system, keeping it quite competitive to the conventional lead-based system. Now that we have designed a potentially optimized cure system based on triazine, and tested it against a typical automotive OEM fuel hose specification, the next step is to make sure that this cure system is suitable for other applications, as well. Designing an injection molded mold 1 n. 1. A hollow form or matrix for shaping a fluid or plastic substance. 2. A frame or model around or on which something is formed or shaped. 3. Something that is made in or shaped on a mold. ECO compound using a triazine cure system Taking the base formulation formulation /for·mu·la·tion/ (for?mu-la´shun) the act or product of formulating. American Law Institute Formulation from our previous work, we can now set up a short experimental design to optimize the triazine system for an injection molded compound, as well. We chose a 2x2x2 Box design with the triazine, CTP and TP being our variables. The HPCA was kept constant because our previous work indicated that too high of loadings of this ingredient would eliminate our scorch safety. For this evaluation, a special combination of MgO, hydrotalcite and calcium carbonate calcium carbonate, CaCO3, white chemical compound that is the most common nonsiliceous mineral. It occurs in two crystal forms: calcite, which is hexagonal, and aragonite, which is rhombohedral. was selected to act as an acid acceptor acceptor - Finite State Machine to neutralize neutralize to render neutral. the HCl that will be given off during the curing reaction. Table 5 shows the experimental design and the parameters used for each variable. We used a least squares method least squares method Statistical method for finding a line or curve—the line of best fit—that best represents a correspondence between two measured quantities (e.g., height and weight of a group of college students). of evaluation and calculated the second order interactions between the main variables. The variables for this experiment were: Rhenogran Triazine TM-70/ECO with a low level of 1.2 phr (- symbol) and a higher level of 1.7 phr (+ symbol), CTP-80 with a lower level of 0.3 phr (-) and a higher level of 0.7 phr (+), along with Rhenogran TP in a 50% active polymeric polymeric /poly·mer·ic/ (pol?i-mer´ik) exhibiting the characteristics of a polymer. pol·y·mer·ic adj. 1. Having the properties of a polymer. 2. dispersion dispersion, in chemistry dispersion, in chemistry, mixture in which fine particles of one substance are scattered throughout another substance. A dispersion is classed as a suspension, colloid, or solution. with a lower level of 0.7 phr (-) and a higher level of 1.3 phr (+). In table 6, the actual results are shown for each of the eight experimental trials, along with the lead-based cure system as a control. All of the experimental trials were mixed and cured using the same laboratory procedures. The raw results show that the proposed new systems generally had equal to better scorch protection, and yet had a faster cure. The original physical properties can easily be matched against the control lead cure system using minimal optimization optimization Field of applied mathematics whose principles and methods are used to solve quantitative problems in disciplines including physics, biology, engineering, and economics. . Heat aging was comparable and compression set was superior to the lead-based cure system, regardless of the change in variables. Oil aging can also be optimized to minimize the tensile loss, and the results indicate less shrinkage Shrinkage The amount by which inventory on hand is shorter than the amount of inventory recorded. Notes: The missing inventory could be due to theft, damage, or book keeping errors. during oil aging than observed in the lead-based control. All of these basic tests indicate that this new Triazine system is quite able to replace the lead-based systems without any major concerns in maintaining performance properties. Additional studies may need to be done to optimize the acid acceptance combination of MgO, CaC[O.sub.3] and hydrotalcite. One of the more important processing aspects of an injection molded compound is its mold flow capabilities. One of the simplest methods to measure the mold flow of a compound is to use a Rheovulcameter (spider mold) to measure the relative differences in mold filling. Each of the nine compounds was tested on the Rheovulcameter with the results shown in table 7. Each of the main variables and second level interactions was evaluated for its effect on the rheovulcameter response. Figure 1 shows the results of the orthogonal At right angles. The term is used to describe electronic signals that appear at 90 degree angles to each other. It is also widely used to describe conditions that are contradictory, or opposite, rather than in parallel or in sync with each other. estimates for the Rheovulcameter response for these variables and secondary interactions. [FIGURE 1 OMITTED] Both the dithiophosphate (ZBPD) and CTP show effects for improving the flow in the spider mold. They also show a positive interaction effect that, when combined with the effect of the main variables, allows us to design a formulation capable of almost matching the mold flow performance of the original lead compound. All three of these effects were found to be significant when checked, with the effect of the ZBPD (Rhenogran TP) having the most influence. The data show that a flow pattern match to the conventional lead cure was almost achieved using the following levels: TMT-70 at 1.7 phr, CTP at 0.7 phr and TP-50 at 1.3 phr (system no. 2). Further testing at higher levels of Rhenogran TP could achieve matching results, based on this preliminary data. Experimental data for chloroprene (ref. 2) Now that we have designed cure systems for ECO for both hose and molded applications, can a similar cure system be made for other chlorinated polymers? Although lead is occasionally used for curing chloroprenes, the use of thioureas in this polymer group is still extensive. Thioureas are also being targeted for potential restriction by several of the automotive OEMs, and could also be banned by the European Union as are lead and the other controlled chemicals. Below is an example of a chloroprene compound cured with a system based on MTT MTT 3-(4,5-Dimethylthiazol-2-Yl)-2,5-Diphenyltetrazolium Bromide MTT Machine Tool Technology MTT Microwave Theory and Techniques MTT Mobile Task Team MTT Multi-Table Tournament (poker) (3-methyl-thiazolidine-thione-2) and Rhenogran HPCA. The conventional cure system used in this example is based on a normal zinc oxide-sulfur system using MBTS MBTS 2-Mercaptobenzothiazyl Disulfide MBTS Missile Bit Test Set MBTS Missile Bench Test Set and TMTD TMTD tetramethylthiuram disulfide. as the accelerators and magnesium oxide magnesium oxide: see magnesia. as the acid acceptor. The proposed system matches the conventional system, without the use of thiourea, lead or other potentially restricted chemicals. In many properties, the new system exceeds the performance of the conventional cure system, including tensile, modulus and properties after aging in hot air for 336 hours at 125[degrees]C (table 8). Conclusions The results of this work illustrate that cost-effective systems can be designed to meet the performance criteria of automotive applications using triazine and similar chemicals, along with selected additives like CTP and Rhenogran HPCA. These formulations are well balanced between the processing parameters and the performance properties, and are capable of being optimized to meet the demanding requirements of injection molding injection molding n. A manufacturing process for forming objects, as of plastic or metal, by heating the molding material to a fluid state and injecting it into a mold. applications. These systems were shown to maintain or improve heat resistance, provide good scorch safety, achieve high physical properties for desired final product performance, and are extremely cost-effective due to their relatively low density compared to the extremely high lead oxides historically used. References (1.) European Directive-2000/53/ELV. (2.) Technical Reports of Rhein Chemie Rheinau GmbH. (3.) "A new optimized system for the lead free crosslinking of epichlorohydrin," a technical report of Rhein Chemie Rheinau GmbH.
Table 1
1 2 3
ECO 100 100 100
Stearic acid 1 1 1
N550 carbon black 50 50 50
Calcium carbonate 5 5 5
Rhenofit D/A 3 3 3
Aflux 54 1 1 1
NDBC 1.05 1.05 1.05
Rhenogran triazine TM-70 1 1 1
Vulkalent E 0.5 1.5
Vulkalent B/C
Rhenogran CTP-80
Mooney viscosity
ML (1+4) 100[degrees]C, 1 day 89 85 89
ML (1+4) 100[degrees]C, 7 days 114 93 91
ML (1+4) 100[degrees]C, 14 days 200 104 88
Physical data
Hardness, A 72 69 No cure
Rebound, % 33 31 No cure
100% modulus, MPa 3.8 2.4 No cure
300% modulus, MPa 9 6.4 No cure
Tensile, MPa 10.80 9.8 No cure
Elongation, % 470 660 No cure
4 5
ECO 100 100
Stearic acid 1 1
N550 carbon black 50 50
Calcium carbonate 5 5
Rhenofit D/A 3 3
Aflux 54 1 1
NDBC 1.05 1.05
Rhenogran triazine TM-70 1 1 1
Vulkalent E
Vulkalent B/C 0.5 1.5
Rhenogran CTP-80
Mooney viscosity
ML (1+4) 100[degrees]C, 1 day 85 81
ML (1+4) 100[degrees]C, 7 days 104 90
ML (1+4) 100[degrees]C, 14 days 200 95
Physical data
Hardness, A 73 71
Rebound, % 32 29
100% modulus, MPa 4 2.7
300% modulus, MPa 8.8 6.7
Tensile, MPa 10.3 9.3
Elongation, % 470 590
6 7
ECO 100 100
Stearic acid 1 1
N550 carbon black 50 50
Calcium carbonate 5 5
Rhenofit D/A 3 3
Aflux 54 1 1
NDBC 1.05 1.05
Rhenogran triazine TM-70 1 1 1
Vulkalent E
Vulkalent B/C
Rhenogran CTP-80 0.5 1.5
Mooney viscosity
ML (1+4) 100[degrees]C, 1 day 79 76
ML (1+4) 100[degrees]C, 7 days 87 81
ML (1+4) 100[degrees]C, 14 days 111 104
Physical data
Hardness, A 71 63
Rebound, % 30 28
100% modulus, MPa 3.4 1.8
300% modulus, MPa 8.5 4.7
Tensile, MPa 10.3 8.3
Elongation, % 490 690
Table 2
ECO masterbatch 162.5 162.5 162.5 162.5 162.5
Triazine TM-70 1 1 1 1 1
CTP-80 1 1 1 1
TP-50 0.5 1 2
Viscosity
ML (1+4), 1 day 89 77 77 75 74
ML (1+4), 7 days 114 83 82 78 75
ML (1+4), 14 days 200 107 92 80 74
Physical data
Hardness, A 72 69 69 70 69
100% modulus, MPa 3.8 2.8 3 3.3 3.1
Tensile, MPa 10.8 9.8 9.9 10.1 9.9
Elongation, % 470 570 590 590 590
Table 3
ECO masterbatch 162.5 162.5 162.5 162.5
[Pb.sub.3][O.sub.4] 4
ETU 1.33
HPCA-70 0 0.5 0.7
Triazine TM-70 1.3 1.3 1.3
CTP-80 0.5 0.5 0.5
TP-50 1 1 1
Viscosity
ML (1+4), 100[degrees]C 77 70 72 74
Mooney scorch, t5 (min.) 5 8.68 6.21 4.53
Mooney scorch, t35 (min.) 8.5 16.9 11.14 6.9
Rheometer,
170[degrees]C, 30 min.
Max-min., Nm 1.13 0.7 1.01 1.19
t10%, min. 0.88 0.9 0.89 0.85
t90%, min. 3.17 5 3.97 2.06
Physical data
Hardness, A 77 72 76 78
Rebound, % 24 22 23 23
100% modulus, MPa 4.8 2.9 4.2 4.8
300% modulus, MPa 15.1 8 12.10 12.60
Tensile, MPa 17.9 13.6 14.3 14.2
Elongation, % 400 630 420 380
Table 4
ECO masterbatch 163 163 163 163
[Pb.sub.3][O.sub.4] 4
ETU 1.33
HPCA-70 0 0.5 0.7
Triazine TM-70 1.3 1.3 1.3
CTP-80 0.5 0.5 0.5
TP-50 1 1 1
Physical data
Hardness, A 77 72 76 78
100% modulus, MPa 4.8 2.9 4.2 4.8 Required
Tensile, MPa 17.9 13.6 14.3 14.2 for fuel
Elongation, % 400 630 420 380 hose
Physical data after
hot air aging
(1,000 hrs C
125[degrees]C)
[delta] Hardness, A +6 +6 +6 +7 +0.00
100% modulus, MPa 7.1 4.9 6.9 7.7
Tensile, MPa 15.8 13.1 13.9 13.3 > 8 Mpa
Elongation, % 215 295 230 170 > 130%
Table 5
Stearic acid 1 1
CB N550 30 30
CB N330 20 20
Aflux 54 (blend 1.5 1.5
of pentaerythrityl
tri- and tetrastearate)
Ether/ester
processing oil 7.5 7.5
Calcium carbonate 5
MgO 2
Hydrotalcite 4
Pb-phosphite-80/ECO 4.5
Pb-phthalate-80/ECO 4.5
NDBC-70/ECO[R] 1.7
ETU-70/ECO 1.7
HPCA 0.5
Triazine TM-70/ECO 1.2-1.7
CTP-80 0.3-0.7
TP-50 (ZBPD) 0.7-1.3
Design TMT/CTP/ZBPD +++
Table 6
Design TMT/CTP/ZBPD Lead +++ -++
Viscosity
ML(1+4), 100[degrees]C 66 65 66
Mooney scorch, t5 (min.) 8.8 10.4 10.3
Mooney scorch, t35 (min.) 17.9 18.3 19.1
Rheometer,
170[degrees]C, 30 min.
Max.-min., Nm 0.92 0.83 0.76
t10, min. 1.05 1.07 1.00
t90, min. 21.5 11.5 12.2
Physical data
Hardness, A 68 71 68
100% modulus, MPa 3.6 4.3 3.9
300% modulus, MPa 10.4 10.6 9.7
Tensile, MPa 12.9 12.1 12.3
Elongation, % 410 380 450
Physical data after hot
air aging (three days
@ 150[degrees]C)
Hardness, A 79 82 79
100% modulus, MPa 6.4 6.3 5.4
Tensile, MPa 11.2 10.6 11.7
Elongation, % 170 170 210
Compression set
24 hrs./
135[degrees]C (VDA) 66 48 49
Physical data after
hot air aging
(1000 hours @
125[degrees]C)
Hardness, A 80 78 77
100% modulus, MPa 6.4 6.1 5.3
Tensile, MPa 10.7 9.2 10.2
Elongation, % 160 145 185
Physical data
after oil aging
(5W40-C20, three
days @ 100[degrees]C)
Hardness, A 70 71 68
Tensile, MPa 13.8 11.4 11.9
Elongation, % 440 310 420
Volume swell, % -3.8 -2 -1.9
Design TMT/CTP/ZBPD --- ++- --+
Viscosity
ML(1+4), 100[degrees]C 67 65 60
Mooney scorch, t5 (min.) 5.5 8.5 9.0
Mooney scorch, t35 (min.) 9.2 15.8 17.1
Rheometer,
170[degrees]C, 30 min.
Max.-min., Nm 0.96 0.89 0.78
t10, min. 0.83 1.03 1.00
t90, min. 8.5 12.4 9.7
Physical data
Hardness, A 71 72 69
100% modulus, MPa 4.1 4.6 3.8
300% modulus, MPa 10.6 11.2 10.2
Tensile, MPa 12.2 11.9 12.4
Elongation, % 380 330 420
Physical data after hot
air aging (three days
@ 150[degrees]C)
Hardness, A 80 80 79
100% modulus, MPa 6.9 7.1 5.9
Tensile, MPa 11.8 11.3 12.4
Elongation, % 170 162 214
Compression set
24 hrs./
135[degrees]C (VDA) 55 56 53
Physical data after
hot air aging
(1000 hours @
125[degrees]C)
Hardness, A 79 80 78
100% modulus, MPa 6.0 6.4 5.1
Tensile, MPa 9.5 9.5 9.2
Elongation, % 150 150 175
Physical data
after oil aging
(5W40-C20, three
days @ 100[degrees]C)
Hardness, A 71 72 69
Tensile, MPa 12.1 12.0 12.3
Elongation, % 370 320 440
Volume swell, % -1.6 -1.6 -2.1
Design TMT/CTP/ZBPD +-- +-+ -+-
Viscosity
ML(1+4), 100[degrees]C 62 61 62
Mooney scorch, t5 (min.) 7.7 10.5 8.7
Mooney scorch, t35 (min.) 13.9 18.4 16.5
Rheometer,
170[degrees]C, 30 min.
Max.-min., Nm 0.89 0.80 0.79
t10, min. 0.95 1.07 0.98
t90, min. 9.8 8.2 11.6
Physical data
Hardness, A 72 72 69
100% modulus, MPa 4.3 4.2 3.7
300% modulus, MPa 11.0 10.4 9.3
Tensile, MPa 11.8 12.0 12.4
Elongation, % 340 380 480
Physical data after hot
air aging (three days
@ 150[degrees]C)
Hardness, A 79 81 79
100% modulus, MPa 6.5 6.6 6.0
Tensile, MPa 10.9 12.5 11.4
Elongation, % 165 190 190
Compression set
24 hrs./
135[degrees]C (VDA) 53 53 58
Physical data after
hot air aging
(1000 hours @
125[degrees]C)
Hardness, A 77 79 76
100% modulus, MPa 6.5 6.1 5.5
Tensile, MPa 9.7 10.3 9.4
Elongation, % 150 165 165
Physical data
after oil aging
(5W40-C20, three
days @ 100[degrees]C)
Hardness, A 72 72 69
Tensile, MPa 11.9 12.0 11.9
Elongation, % 320 340 430
Volume swell, % -2.2 -2.1 -1.7
Table 7
1 2 3
Design TMT/CTP/ZBPD Lead +++ -++
Rheovulcameter
100/170[DEGREES]C
Injection volume,
[mm.sup.3] 1,890 1,610 1,600
After cool storage
2w, [mm.sup.3] 1,047 725 835
Injection speed,
[mm.sup.3]/s 87 73 71
After cool storage
2w, [mm.sup.3]/s 137 94 109
4 5 6
Design TMT/CTP/ZBPD --- ++- --+
Rheovulcameter
100/170[DEGREES]C
Injection volume,
[mm.sup.3] 1,180 1,470 1,690
After cool storage
2w, [mm.sup.3] 440 490 380
Injection speed,
[mm.sup.3]/s 51 64 75
After cool storage
2w, [mm.sup.3]/s 58 64 51
7 8 9
Design TMT/CTP/ZBPD +-- +-+ -+-
Rheovulcameter
100/170[DEGREES]C
Injection volume,
[mm.sup.3] 1,440 1,560 1590
After cool storage
2w, [mm.sup.3] 420 420 465
Injection speed,
[mm.sup.3]/s 64 67 70
After cool storage
2w, [mm.sup.3]/s 56 56 60
Table 8
Alternative
Compound Conventional cure
CR master 160 phr 160 phr
MgO 5 0
ZnO 5 5
Sulfur 0.2 0
M BTS 1.5 0
TMTD 0.8 0
MTT 0 1.5
Rhenogran HPCA 0 3
Physical properties
Cured 160[degrees]/T90
Tensile, MPa 11.5 14.8
Elongation, % 660 470
Hardness A 64 66
Monsanto fatigue
80% elongation, KC 391 410
100% elongation, KC 314 322
Aged 336 hours Q 125[degrees]C
Elongation change, % -80 -63
100% modulus change, % +290 +112
Hardness A change +24 +14
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